EP1380639B1 - Procede de fabrication d'une solution eau-alcool - Google Patents

Procede de fabrication d'une solution eau-alcool Download PDF

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Publication number
EP1380639B1
EP1380639B1 EP02797001A EP02797001A EP1380639B1 EP 1380639 B1 EP1380639 B1 EP 1380639B1 EP 02797001 A EP02797001 A EP 02797001A EP 02797001 A EP02797001 A EP 02797001A EP 1380639 B1 EP1380639 B1 EP 1380639B1
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EP
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Prior art keywords
water
alcohol
aqueous
alcoholic
acid
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EP02797001A
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German (de)
English (en)
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EP1380639A1 (fr
EP1380639A8 (fr
EP1380639A4 (fr
Inventor
Valery Nikolaevich Sorokin
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000 "Naucho-Proizvodstvennoe Obiedinenie "Opytnay A Vodno-Analiticheskaya Laboratoria
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000 "Naucho-Proizvodstvennoe Obiedinenie "Opytnay A Vodno-Analiticheskaya Laboratoria
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Priority claimed from RU2002100464A external-priority patent/RU2216582C2/ru
Priority claimed from RU2002100465A external-priority patent/RU2216583C2/ru
Priority claimed from RU2002107883/13A external-priority patent/RU2243992C2/ru
Priority to EP09075163A priority Critical patent/EP2130900A1/fr
Application filed by 000 "Naucho-Proizvodstvennoe Obiedinenie "Opytnay A Vodno-Analiticheskaya Laboratoria filed Critical 000 "Naucho-Proizvodstvennoe Obiedinenie "Opytnay A Vodno-Analiticheskaya Laboratoria
Publication of EP1380639A1 publication Critical patent/EP1380639A1/fr
Publication of EP1380639A8 publication Critical patent/EP1380639A8/fr
Publication of EP1380639A4 publication Critical patent/EP1380639A4/fr
Publication of EP1380639B1 publication Critical patent/EP1380639B1/fr
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Priority to CY20091101291T priority patent/CY1109574T1/el
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Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36—Carboxylic acids; Salts or anhydrides thereof
    • A61K8/362—Polycarboxylic acids
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
    • A61K47/08—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing oxygen, e.g. ethers, acetals, ketones, quinones, aldehydes, peroxides
    • A61K47/10—Alcohols; Phenols; Salts thereof, e.g. glycerol; Polyethylene glycols [PEG]; Poloxamers; PEG/POE alkyl ethers
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34—Alcohols
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36—Carboxylic acids; Salts or anhydrides thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783—Angiosperms [Magnoliophyta]
    • A61K8/9789—Magnoliopsida [dicotyledons]
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/0012—Galenical forms characterised by the site of application
    • A61K9/0014—Skin, i.e. galenical aspects of topical compositions
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12G—WINE; PREPARATION THEREOF; ALCOHOLIC BEVERAGES; PREPARATION OF ALCOHOLIC BEVERAGES NOT PROVIDED FOR IN SUBCLASSES C12C OR C12H
    • C12G3/00—Preparation of other alcoholic beverages
    • C12G3/04—Preparation of other alcoholic beverages by mixing, e.g. for preparation of liqueurs
    • C12G3/05—Preparation of other alcoholic beverages by mixing, e.g. for preparation of liqueurs with health-improving ingredients, e.g. flavonoids, flavones, polyphenols or polysaccharides
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12G—WINE; PREPARATION THEREOF; ALCOHOLIC BEVERAGES; PREPARATION OF ALCOHOLIC BEVERAGES NOT PROVIDED FOR IN SUBCLASSES C12C OR C12H
    • C12G3/00—Preparation of other alcoholic beverages
    • C12G3/04—Preparation of other alcoholic beverages by mixing, e.g. for preparation of liqueurs
    • C12G3/06—Preparation of other alcoholic beverages by mixing, e.g. for preparation of liqueurs with flavouring ingredients
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/85—Products or compounds obtained by fermentation, e.g. yoghurt, beer, wine

Definitions

  • the present invention relates to the field of food industry, where it may be used for producing alcoholic products, to pharmacology for producing infusions tinctures and extracts or preparations containing aqueous-alcoholic solutions as pharmaceutically acceptable media and also to cosmetology for producing cosmetic products containing aqueous-alcoholic solutions as cosmetically acceptable media.
  • Aqueous-alcoholic solutions are products in great demand in various fields of the art. This especially concerns production of a broad range of alcoholic products, production of infusions and extracts employed in pharmacology, which contain biologically active ingredients, production of various cosmetic products.
  • the demand for said solutions stimulates constant improvements in their properties used in some product or other. It is desirable that the technology of making the product whose component part is an aqueous-alcoholic solution should undergo insignificant changes, this also fully applying to the procedure of preparing the aqueous-alcoholic solution as such.
  • distillery products are divided into 15 groups: liqueurs (strong, dessert, emulsion), cremes, cordials, punches, infusions (sweet, semi-sweet, semi-sweet low alcohol, bitter, bitter low-alcohol), dessert beverages, aperitifs, balsams and cocktails ( V.M. Poznyakovskij (Ed.), "Ekspertiza Napitkov” (Examination of Beverages), Novosibirsk: Novosibirsk University Publishers, 1999, p. 63 (1) (in Russian ); " Pishchevaya Promyshlennost'", Moscow, 2001, No. 6, pp. 63, 63 ; “Pishchevaya Tekhnologiya”, Moscow, 2000, No. 5, p. 70 (in Russian ).
  • compositions of multicomponent beverages have been formulated mainly by way of empirical selection of ingredients, whose apt ratio is estimated by experts.
  • an approach has been empirically developed, which makes it possible to systematize the results of investigations and simulate the properties of products being developed: constructing a model of the properties of a multicomponent mixture, based on the results of expert evaluation of alternatives, may be successfully used for determining the best beverage formulation ( Izvestiya Vuzov, "Pishchevaya Tekhnologiya", Krasnodar, 2001, No. 1, pp. 57-59 (in Russian )).
  • an aqueous-alcoholic solution is used, prepared by blending high-purity rectified alcohol with corrected purified potable water.
  • aqueous-alcoholic beverages having a strength of 12-60% are produced by blending preliminarily prepared semi-finished components: infusions, juices, aromatic alcohols, alcoholic solutions of ethereal oils with extra-purity rectified ethyl alcohol and conditioned potable water, and ripening the blend.
  • Water conditioning comprises a number of purification operations, depending on the quality of starting water: filtering through sand or ceramic filters, coagulation, settling, filtering through sand filters, softening by passing through ion-exchange resins (e.g., through a sodium cation-exchanger) or by a reverse osmosis water treatment with the help of semi-permeable membranes (ibidem, p. 26).
  • ion-exchange resins e.g., through a sodium cation-exchanger
  • a reverse osmosis water treatment e.g., a reverse osmosis water treatment with the help of semi-permeable membranes (ibidem, p. 26).
  • High-purity aqueous-alcoholic solutions used for the above-indicated purposes are prepared by blending rectified ethyl alcohol and purified potable water.
  • the technology of purifying and preparing water for bottling described in the journal " Pishchevaya Promyshlennost' '', 2001, No. 3, p. 66 , actually takes into account most of the latest achievements and comprises, if necessary, 7 steps:
  • the water thus prepared corresponds to the main threshold limit values (color, hydrogen ion exponent, turbidity, content of iron, sulfates, sodium and potassium, total hardness).
  • Patent RU 2133266 contemplates producing an aqueous-alcoholic mixture from alcohol of "Extra" grade and potable water with hardness not exceeding 0.36 mg-equiv./liter.
  • the employed water is clarified with alumina and softened with the help of sodium cation exchanger.
  • the method contemplates filtering an aqueous-alcoholic solution through a 4-meter high layer of activated carbon BOW and through sand filters with the rate of 40 dal/hr on fresh carbon and 30 dal/hr on regenerated carbon.
  • the process contemplates also introducing into the aqueous-alcoholic solution sugar dissolved in water (in the production of vodka).
  • patent RU No. 2130056 in the production of special ("osobaya”) vodka, with a view to lowering the cost price while preserving the organoleptic properties of the target product, it is proposed to use for preparing an aqueous-alcoholic solution highest-purification rectified alcohol and softened water which has passed trough a sand filter and a carbon column on a fresh filter with carbon activity of at least 15 units.
  • an aqueous-alcoholic solution is prepared by blending rectified ethyl alcohol with purified potable water, followed by purifying the aqueous-alcoholic solution by modified starch; further, in the course of producing vodka in a finishing vat, the aqueous-alcoholic solution is added with a mixture of sugar in the form of its aqueous solution or a syrup with lactose (1.8-2.2 kg) and citric acid (0.2-0.4 kg per 1000 dal of finished product), preliminarily dissolved in purified water and kept for 20-24 hours at a temperature of 15-25°C.
  • patent RU No. 2166537 which discloses a vodka production process, into a filtered aqueous-alcoholic solution a mixture of a sweetener with tartaric and ascorbic acids is added, in the following amounts: tartaric acid, 0.1-0.3 kg; ascorbic acid, 0.09-0.15 kg; and sugar substitute, 0.1-0.15 kg per 1000 dal of finished product.
  • an aqueous-alcoholic solution (for vodka production) is prepared by blending rectified ethyl alcohol with potable water treated by reverse osmosis, filtering the aqueous-alcoholic solution through active carbon and subsequent introducing an aqueous-alcoholic infusion of flax seeds in the course of blending ethyl alcohol with the treated water, and introducing a mixture of fructose and ascorbic acid at the final step of vodka production (5.5-6.5 kg of fructose and 0.04-0.06 kg of ascorbic acid per 1000 dal of vodka).
  • the main processes for preparing aqueous-alcoholic solutions and products based thereon are physicochemical processes of adsorption, diffusion and dissolution.
  • the first two of said processes are widely used in the practice of preparing aqueous-alcoholic liquids and products therefrom, which cannot be said about the process of dissolution - mutual dissolution of alcohol and water, about the dissolution or non-dissolution (precipitation) of admixtures present in both the starting water and alcohol and forming in the process of their blending.
  • volatile admixtures more than 70 various compounds were found, including higher alcohols that have bitter taste and sharp fusel smell, fusel oil alcohols, including n-propyl alcohol, n-butyl alcohol, n-amyl alcohol, etc., up to nonyl alcohol, as well as iso-alcohols corresponding to the above-said alcohols, mainly, isoamyl and isobutyl ones; aldehydes (acetaldehyde, formaldehyde, butyraldehyde, propionaldehyde, isovaleraldehyde, crotonic aldehyde, furfural, and others); ketones; esters (mainly ethyl acetate); acids (acetic, propionic, butyric, and others).
  • fusel oil alcohols including n-propyl alcohol, n-butyl alcohol, n-amyl alcohol, etc.
  • iso-alcohols corresponding to the above-said alcohols, mainly,
  • an aqueous-alcoholic solution is prepared by blending rectified ethyl alcohol with softened potable water, followed by purification of the resulting aqueous-alcoholic solution by passing it through a carbon cleansing battery, and filtration. Blending of alcohol and water is performed under turbulence conditions with the components moving in counterflow in a "pipe in the pipe” type mixer or in a special mixer of alcohol and water flows in a volume ratio of 1:1.38-1.44. Purification of the aqueous-alcoholic solution with active carbon is carried out under fluidized bed conditions.
  • Filtration is carried out in three steps: first in a hydrocyclone, then through coarse frame flannel filters, and finally through a fine filter (hydrocompressed layer of quartz sand).
  • the creation of turbulence owing to the counterflow provides favorable hydrodynamic conditions for mixing and dissolution of the alcohol in the water.
  • Patent RU No. 2169185 does not teach anything new about mixing under turbulence conditions. It is noted only that blending is carried out in a mixer till complete dissolution of alcohol in water.
  • patent RU No. 2124353 discloses a topical pharmaceutical composition for skin treatment and care, which comprises in a cosmetically acceptable medium, namely, in an aqueous-alcoholic solution, at least one product with an irritant side effect.
  • Patent RU No. 2174388 teaches "Aromatizing and Refreshing Composition" comprising monomenthyl succinate in a cosmetically acceptable liquid - an aqueous-alcoholic solution. Furthermore, it is proposed to use this composition for preparing alcoholic beverages as well.
  • Aqueous-alcoholic solutions are also used as self-contained medicinal preparations (numerous tinctures, extracts and their combinations) ( M. Palov, "Encyclopedia of Medicinal Plants", Russian translation by “Mir”, Moscow, 1988 ) .
  • the aqueous-alcoholic solution is prepared by blending a rectified highest-purity alcohol or "Extra” grade or “De luxe” grade alcohol with potable water (deodorized and softened) in a small-volume annular apparatus, wherein, due to the high turbulence of flow, optimal conditions for the alcohol dissolution are created.
  • It is an object of the present invention is to provide a new process for preparing aqueous-alcoholic solutions of better quality by enhancing the dynamicity of solutions and ruling out warming up of the mixture of ethyl alcohol and water when blending thereof.
  • Another object of the present invention is to simplify the preparation of aqueous-alcoholic solutions by excluding the step of purifying the solution after blending.
  • Said objects are accomplished by that in a process for preparing an aqueous-alcoholic solution by blending purified potable water with rectified ethyl alcohol, which comprises a filtering step, before blending water with alcohol, a separate protonation of water and alcohol is carried out, followed by filtering the water and alcohol.
  • An additional, third object of the invention is to prepare aqueous-alcoholic solutions of better quality by raising the effectiveness of separate protonation of water and alcohol before blending thereof, owing to additional protonation carried out by intermixing separate flows of protonated water and protonated alcohol in glass or porcelain vessels, using glass or porcelain stirrers; respectively.
  • Still another object of the invention is to speed-up the process for preparing aqueous-alcoholic beverages with better physicochemical characteristics and organoleptic properties and, as a consequence, to make the technological process of preparing aqueous-alcoholic beverages cheaper.
  • This object is accomplished by that in a process for preparing an aqueous-alcoholic beverage, which comprises preparing semi-finished products and blending semi-finished products with high-purity rectified ethyl alcohol and conditioned potable water, followed by ripening the blend, separately protonated and filtered alcohol and water are used.
  • protonation of water is carried out by introducing into water proton donors stronger than water, particularly inorganic acids, preferably orthophosphoric acid or carbonic acid, in an amount of 0.05-0.2 wt.%.
  • Protonation of ethanol is carried out by introducing acids stronger than ethanol as the proton donors.
  • acids stronger than ethanol either organic or inorganic acids can be used, preferably hydrochloric acid or citric acid or ascorbic acid or oxalic acid, in an amount of 0.1-0.5 wt.%.
  • Boundary amounts of the introduced additives are determined by that when the amounts are lower than indicated above, an excess of protons is formed in the system, which is not sufficient for preventing warming-up of the aqueous-alcoholic mixture, while introducing additives in amounts exceeding the claimed values may adversely affect the organoleptic characteristics of products.
  • Separate filtering of protonated alcohol and protonated water may be effected, for example, by using reverse osmosis and Na-cationization technology.
  • the set object is accomplished by that in a process for preparing an aqueous-alcoholic solution based on purified potable water and rectified ethyl alcohol, which comprises separate protonation of water by introducing thereinto 0.05-0.2 wt.% of proton donors stronger than water and separate protonation of ethyl alcohol by introducing thereinto 0.1-0.5% of proton donors stronger than ethyl alcohol; separate filtering of the protonated water and ethyl alcohol, and blending thereof, the protonated water and water, before filtering are directed in separate flows into two cylindrical glass or porcelain vessels, wherein they are intermixed for 1-5 min with the help of glass or porcelain stirrers, respectively, rotated with the speed of preferably 1000-3000 rpm.
  • a stirrer of any type: paddle mixer, impeller mixer or anchor stirrer can be used, a paddle mixer with one or more paddles secured to the mixer axle being preferable.
  • the set object is accomplished by that in a process for preparing an aqueous-alcoholic beverage, which comprises preparing semi-finished products and blending the semi-finished products with purified rectified ethyl alcohol and conditioned potable water, followed by ripening the blend, separately protonated and filtered alcohol and water are used.
  • 0.1-0.5 wt.% of proton donors stronger than alcohols is introduced thereinto, for instance, organic or inorganic acids, such as hydrochloric acid, citric acid, ascorbic acid, oxalic acid;
  • organic or inorganic acids such as hydrochloric acid, citric acid, ascorbic acid, oxalic acid;
  • water 0.05-0.2 wt.% of proton donors stronger than water is introduced thereinto, for instance, an inorganic acid, preferably orthophosphoric acid or carbonic acid.
  • the source of semi-products are various kinds of vegetable stock.
  • so called blending materials are used: sugar, honey, acids (including ascorbic acid and citric acid), colorants, etc.
  • Alcoholized juices are prepared from comminuted stock by squeezing juice out of it and then preserving the juice with rectified alcohol to a strength of about 26% or with using alcololized fruit juices, settling, and filtering.
  • Alcoholized fruit juices are prepared by two- and more-fold steeping of fresh or dried fruit-and-berry stock with an aqueous-alcoholic solution.
  • Alcoholized infusions are produced according to a similar technology by steeping lemon or orange peel, herbs, nuts, and the like.
  • One kind of stock or a mixture of various components can be subjected to extraction, e.g., for preparing balsam infusions.
  • the total duration of the processes is from 4-8 to 10-20 days.
  • First- and second-decantation infusions and fruit juices are combined and filtered.
  • Aromatic alcohols comprising products of distillation with water-alcohol vapors of volatile aromatics from essential oil-bearing plant or fruit-and-berry stock, and also from semi-products based on this stock, are prepared by charging the stock into the distillation still of the apparatus and covering the stock with a 45-60% aqueous-alcoholic solution, and after short-time steeping distillation is carried out.
  • Aromatic alcohols can be prepared from fruit juices and infusions.
  • Ethereal oils are extracted with solvents from plant stock, the solvent being then distilled-off.
  • Sugar syrup used for preparing a blend has the 65.8% concentration of dry substances for most distillery products and 73.2% for liqueurs.
  • the blend is prepared in collecting vessels, the ingredients being fed thereto in a definite sequence according to branch instructions.
  • the blend is collected, then its physicochemical characteristics are checked and corrected, if required, by introducing lacking ingredients.
  • blends are ripened for 24-72 hours.
  • Examples 1-3 are carried out using citric acid as the most preferable proton donor for alcohol in amounts of from 0.1 to 0.5 wt.% and using carbon acid as the proton donor for water in an amount of 0.05-0.2 wt.%. Said amounts of both donors are also preferable ones.
  • the alcohol to water ratio is selected such that the strength of the obtained aqueous-alcoholic solutions (alcohol concentration in volume percent) should be from 10 vol.% to 40 vol.%, this corresponding to beverages ranging from low-alcoholic ones to vodkas, though the process may be successfully used to both weaker and stronger beverages.
  • Examples 4 and 5 carried out similarly to Examples 1-3 but with the use of other proton donors, support the attaining of stable advantages offered by the proposed process in a broad range of alcohol concentrations: from 4 vol.% to 40 vol.%.
  • the upper limit of 40 vol.% can be accounted for by the fact that the quality characteristics of 40% solutions can be compared with the GOST ratings established for vodkas (40% aqueous-alcoholic solutions).
  • Table 1 Listed in Table 1 are also GOST ratings and the data of control Example 6 which was carried out without introducing proton donors into alcohol and water separately, but with carrying out adsorption with active carbon and double filtration - before and after blending water with alcohol (conventional process of preparing aqueous-alcoholic solutions).
  • Examples 7-9 illustrate the process in accordance with the invention, i.e., the preparation of aqueous-alcoholic solutions with the use of various (preferable) proton donors for alcohol and water, taken in the claimed (preferable) ratios, subjected to additional protonation carried out by intensive intermixing of protonated flows of alcohol and water, directed separately to cylindrical glass or porcelain vessels, using glass or porcelain stirrers respectively; the intermixing is performed during different periods of time and with different rotation speeds of the stirrers (preferable values of these parameters are presented).
  • Examples 10-11 are control ones: in Example 10 additional protonation is carried out in a stainless steel vessel with a stirrer from the same material; in Example 11 a stainless steel vessel and a stirrer made from glass are used.
  • control Example 12a control Example 12a
  • analogous data obtained in accordance with the invention Example 12b: the technology of preparing finished products is identical with the control, but contemplates the use of preliminarily protonated and filtered alcohol and water (sodium-cationization or reverse osmosis).
  • a 25% strong lemon liqueur is prepared on the basis of an aromatic alcohol extracted from fresh lemon peel (180 kg) with the content of ethereal oil in the stock equal to 4.05 liter. Distillation with a 60% aqueous-alcoholic liquid (90 dal) gave 54 dal of 75% aromatic alcohol with the content of ethereal oil of 0.56 ml in 100 ml, the total content of the ethereal oil in the aromatic alcohol being 3 liters.
  • composition of blend (in liters per 1000 dal) : Aromatic alcohol from lemon peel, containing 3 liters of ethereal oil 607.5 66% sugar syrup 5156.0 Highest-purity (96.2%) rectified ethyl alcohol 2125.10 Softened potable water to make the volume equal to 1000 dal.
  • the total time of preparing liqueurs is from 10 to 28 hours (p. 303).
  • Organoleptic characteristics gold-colored liqueur with sweet taste and lemony aroma.
  • Aromatic alcohol in the amount of 0.61 liter is obtained, starting from 0.122 kg of fresh lemon peel and 1.020 kg of a 60% aqueous-alcoholic solution of 96.2% ethyl alcohol: the aqueous-alcoholic solution contains 483 g of alcohol and 537 g of water.
  • the ethyl alcohol is protonated by adding 0.15 wt.% (0.72 g) of ascorbic acid and filtered (sodium-cationization and reverse osmosis); water is preliminarily protonated by adding 0.1 wt.% (0.54 g) of orthophosphoric acid and filtered (sodium-cationization and reverse osmosis).
  • ethyl alcohol For bringing the total volume of the blend to 1 dal (10 liters) 2.125 liters of 96.2% ethyl alcohol are required, this corresponding to 1.73 kg; the required amount of water is 2.065 liters (2.065 kg).
  • Preliminary protonation of ethyl alcohol before preparing the blend is carried out by introducing 0.15 wt.% (2.6 g) of ascorbic acid and filtering (sodium-cationization and reverse osmosis); water is preliminarily protonated by introducing 0.1 wt.% (2.065 g) of orthophosphoric acid and filtered (sodium-protonation and reverse osmosis).
  • Total time of preparing the liqueur is 5-7 hours.
  • the liqueur thus produced is characterized by a more saturated color, fine aroma of lemon, and tastes sweet.
  • Examples 13-15 illustrate the use of aqueous-alcoholic solutions prepared in accordance with the proposed process in pharmaceutics and cosmetology, wherein aqueous-alcoholic solutions are widely employed for the preparation of infusions, tinctures, extracts and various medicaments for external use. Said products always contain active ingredients, which basically determine their characteristics. Aqueous-alcoholic solutions therein play mainly the role of pharmaceutically and cosmetically acceptable media.
  • Example 13 a) Control. Preparing a valerian tincture producing sedative and regulatory effect on the cardiovascular system.
  • Comminuted and dried roots and rhizomes of valerian are wetted in a vessel provided with a ground stopper with a sufficient amount of a 60% aqueous-alcoholic solution (prepared on the basis of 96.2% ethyl alcohol). 5 hours later the swollen material is tightly stowed in a percolator with the drain valve open, adding such an amount of the aqueous-alcoholic solution that its layer above the surface of the material should be 35 mm. The liquid flown from the drain valve is poured back into the percolator, the drain valve is closed, and the percolator is allowed to stand for 24 hours. After that the percolation process is carried out slowly, so that during 1 minute 20 drops of the liquid should flow out. The percolate is collected and brought to the required volume with the same solvent. The total consumption of the aqueous-alcoholic solution was 1 kg.
  • valerian tincture is prepared, using an aqueous-alcoholic solution prepared from separately protonated and filtered alcohol and water.
  • the amount of alcohol in the solution is 473 g and the amount of rater is 527 g.
  • the protonation of alcohol is effected by adding 0.15 wt.% (0.7 g) of ascorbic acid; the protonation of water is effected by adding 0.1 wt.% (0.53 g) of orthophosphoric acid.
  • Control The preparation of a dentifrice water - a means for rinsing out the mouth after cleaning the teeth and food intake, which has not only hygienic, but also curative and prophylactic properties (strengthening of the gingivae and decreasing gingival hemorrhage.
  • a vessel with a 2 g batch of propolis is placed on a water bath for 15 minutes. Then slowly, during 10 minutes a 0.02 g batch of menthol is transferred thereto, thoroughly intermixing the contents with a glass rod. The mixture is cooled. Then added portion-wise to the vessel with the mixture of propolis and menthol, while stirring thoroughly, is an aqueous-alcoholic solution containing 31 g of ethyl alcohol of "Extra" grade and 66.96 g of water, and the contents are thoroughly intermixed for another 40 minutes. The mixture is left to stand for 24 hours.
  • the dentifrice water thus prepared is a homogeneous transparent light-brown liquid with a pleasant odor.
  • Clinical experimental investigations have revealed a disinfecting and anti-inflammatory effect of the dentifrice water. This dentifrice water does not produce allergizing or irritating effect.
  • a dentifrice water is prepared from a protonated aqueous-alcoholic solution.
  • the latter is prepared from 31 g of ethyl alcohol "Extra" preliminarily protonated with 0.1 wt.% (0.03 g) of citric acid and 66.98 g of purified water preliminarily protonated with 0.1 wt.% (0.067 g) of carbonic acid.
  • the preliminarily protonated alcohol and water are additionally protonated by stirring separately alcohol and water in cylindrical glass vessels for 3 minutes with the help of glass stirrers rotating with the speed of 2000 rpm. After that filtering is performed by using sodium-cationization and reverse osmosis technologies.
  • the preparation of the dentifrice water analogous in its effectiveness to the dentifrice water according to Example 14a required twice less time (12 hours) for letting the mixture stand.
  • Control The preparation of a cosmetic composition (lotion) for face care, which cleanses the skin and stimulates blood circulation.
  • a lotion is prepared, containing 3 wt.% (3 g) of natural rose oil, 30 wt.% (30 g) of ethyl alcohol "Extra” and 67 wt.% (67 g) of purified water.
  • an alcoholic solution of the aromatic ethereal oil is formed with the weight oil/alcohol ratio of 1:8; then to the resulting mixture an aqueous-alcoholic solution is added, comprising the rest of the alcohol and all the water.
  • the obtained emulsion is filtered through a polymeric membrane.
  • the obtained filtrate comprises a lotion which has an odor of rose oil, cleanses, softens and produces tonic effect on the skin.
  • a lotion is prepared by following the above procedure, but preliminarily alcohol and water are subjected separately to protonation.
  • alcohol 0.3 wt.% (0.09 g) of oxalic acid is used, for the protonation of water 0.1 wt.% (0.067 g) of carbonic acid is used.
  • the lotion thus prepared is characterized by improved softening properties owing to deeper penetration of the protonated liquid into skin integument.
  • the proposed process not only provides the possibility of preparing alcoholic beverages and pharmaceutical and cosmetic products of improved quality, but also to shorten the production cycle in the case of preparing infusions and tinctures (by as much as two times and more) and, as a consequence, to cut down the product costs.
  • Such considerable positive effect has become achievable owing to the principally new approach to the solving the general physicochemical problem of preparing aqueous-alcoholic solutions.
  • Aqueous-alcoholic solutions prepared in accordance with the proposed process may be widely used in alcoholic beverage industry in making low-alcohol products; they may find application in pharmacology in making preparations in the form of aqueous-alcoholic solutions, infusions, tinctures and extracts, and also in cosmetic industry as cosmetically acceptable media, since the requirements to aqueous-alcoholic solutions to be used for the indicated purposes are analogous. In all the cases of using protonated aqueous-alcoholic solutions their main effect - reduced toxicity - is provided.

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Claims (9)

  1. Procédé pour produire une solution aqueuse-alcoolique comprenant des étapes de
    a) faire une protonation séparée d'eau potable purifiée avec un donneur de protons plus fort que de l'eau choisi à partir d'un groupe comportant de l'acide orthophosphorique et de l'acide carbonique dans la quantité de 0,05 à 0,2% en poids et d'éthanol rectifié avec un donneur de protons plus fort que l'alcool choisi à partir d'un groupe comportant de l'acide chlorhydrique, de l'acide citrique, de l'acide ascorbique, de l'acide oxalique dans la quantité de 0,1 à 0,5% en poids,
    b) faire une filtration séparée des produits cibles obtenus à l'étape a) en utilisant la technique d'échange de cations de sodium et d'osmose inverse,
    c) mélanger les produits filtrés obtenus à l'étape b).
  2. Procédé selon la revendication 1, qui comprend de plus l'étape de protonation, mise en oeuvre avant l'étape b), lorsque l'eau potable et l'alcool d'éthyle protonatés sont dirigés en écoulements séparés vers deux récipients en verre ou en porcelaine cylindriques, dans lesquels les écoulements se mélangent à l'aide d'agitateurs réalisés en verre et en porcelaine, respectivement.
  3. Procédé selon la revendication 2, dans lequel ledit mélange est mis en oeuvre pendant approximativement 1-5 minutes.
  4. Procédé selon la revendication 2, dans lequel ledit mélange est mis en oeuvre avec les agitateurs tournant à une vitesse d'approximativement 1000-3000 tours par minute.
  5. Procédé selon la revendication 1, dans lequel un semi-produit préparé sur la base d'un bouillon de légumes est ajouté.
  6. Procédé selon la revendication 5, dans lequel le semi-produit est préparé avec l'utilisation d'une solution aqueuse-alcoolique préparée selon la revendication 1 ou 2.
  7. Procédé selon la revendication 5, dans lequel ledit semi-produit comprend du bouillon de légumes frais ou en poudre, un jus alcoolisé, un jus de fruit, une infusion ou teinture, et une huile essentielle.
  8. Procédé selon la revendication 5, qui comprend de plus au moins une matière d'apport.
  9. Procédé selon la revendication 8, dans lequel ladite matière d'apport comprend du sucre sous forme de sirop.
EP02797001A 2002-01-15 2002-12-23 Procede de fabrication d'une solution eau-alcool Expired - Lifetime EP1380639B1 (fr)

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EP09075163A EP2130900A1 (fr) 2002-01-15 2002-12-23 Procédé de préparation d'une solution hydroalcoolique
CY20091101291T CY1109574T1 (el) 2002-01-15 2009-12-09 Μεθοδος παραγωγης ενος διαλυματος νερου-αλκοολης

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RU2002100465 2002-01-15
RU2002100464A RU2216582C2 (ru) 2002-01-15 2002-01-15 Способ получения водно-спиртового раствора и алкогольный, фармацевтический и косметический продукты, изготовленные с его использованием
RU2002100465A RU2216583C2 (ru) 2002-01-15 2002-01-15 Способ получения водно-спиртового напитка и водно-спиртовый напиток
RU2002100464 2002-01-15
RU2002107883 2002-03-28
RU2002107883/13A RU2243992C2 (ru) 2002-03-28 2002-03-28 Способ получения водно-спиртового раствора и алкогольный, фармацевтический и косметический продукты, изготовленные с его использованием
PCT/RU2002/000547 WO2003062368A1 (fr) 2002-01-15 2002-12-23 Procede de fabrication d'une solution eau-alcool et produits fabriques a base de cette solution

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EP1380639A1 EP1380639A1 (fr) 2004-01-14
EP1380639A8 EP1380639A8 (fr) 2004-06-02
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EP1380639B1 true EP1380639B1 (fr) 2009-09-09

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DE102009041753A1 (de) * 2009-09-16 2011-03-24 Bionorica Se Wasch-, Reinigungs- oder Desinfektionsmittel enthaltend Hydrolysate aus Pflanzenextrakten
WO2011088420A1 (fr) * 2010-01-15 2011-07-21 Ocean Spray Cranberries, Inc. Procédé d'extraction d'un composé de feuilles de canneberge et produits apparentés
US20110318468A1 (en) * 2010-06-29 2011-12-29 Aleksandre Kakhaberi Fructose-based anti-diabetic alcoholic beverage and method of making same
CN103131619A (zh) * 2013-02-26 2013-06-05 郑海鸿 葡萄酒饮品及其制备方法
GB2534585A (en) * 2015-01-28 2016-08-03 Smith & Sinclair Ltd A confectionery composition and a method of manufacturing thereof
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US20100240771A1 (en) 2010-09-23
US7750052B2 (en) 2010-07-06
ES2333111T3 (es) 2010-02-17
IL157884A0 (en) 2004-03-28
EP1380639A1 (fr) 2004-01-14
US20040109900A1 (en) 2004-06-10
JP2005514943A (ja) 2005-05-26
CN1620496A (zh) 2005-05-25
DE60233651D1 (de) 2009-10-22
EP1380639A8 (fr) 2004-06-02
PT1380639E (pt) 2009-11-23
CA2473283A1 (fr) 2003-07-31
EP2130900A1 (fr) 2009-12-09
CN1620496B (zh) 2010-06-23
EP1380639A4 (fr) 2004-06-16
CY1109574T1 (el) 2014-08-13
WO2003062368A1 (fr) 2003-07-31
EA200300868A1 (ru) 2004-08-26
ATE442431T1 (de) 2009-09-15
DK1380639T3 (da) 2009-12-21
EA006862B1 (ru) 2006-04-28

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